関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methoxyacetic Acid | HCID 12251 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | 2-(3-(3,4-Dichlorophenyl)-4-aminobutyl)oxytetrahydropyran | HCID 15670808 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-methoxyacetyl-2-(3,4-dichlorophenyl)-4-(tetrahydropyran-2-yloxy)butylamin | HCID 19705334 | 71.1% |
反応手順
A mixture of 8.6 g of 2-(3,4-dichlorophenyl)-4-(tetrahydropyran-2-yloxy)butylamine (obtained according to PREPARATION (I), step (b)), 2.46 g of methoxyacetic acid, 5.55 g of triethylamine in 50 ml of dichloromethane is cooled to 0° C. and 14.5 g of BOP is added thereto. The reaction mixture is stirred for one hour at room temperature and concentrated under vacuum. The residue is taken up in ethyl acetate and is successively washed with water, dried over Na2SO4 and concentrated under vacuum. The residue is chromatographed on silica gel using CH2Cl2/CH3OH (100/1 v/v) as the eluent to give 7.5 g of the expected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05554763 |
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| 出典データセット | uspto-grants-1996_09 |
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| ORD ID | ord-0c8ce3533d57469fb98ac376e471eabf |
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| 出典メモ | uspto-grants-1996_09 |
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